JP4230541B2 - Binder removal method - Google Patents
Binder removal method Download PDFInfo
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- JP4230541B2 JP4230541B2 JP53062998A JP53062998A JP4230541B2 JP 4230541 B2 JP4230541 B2 JP 4230541B2 JP 53062998 A JP53062998 A JP 53062998A JP 53062998 A JP53062998 A JP 53062998A JP 4230541 B2 JP4230541 B2 JP 4230541B2
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- Prior art keywords
- binder
- article
- water
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- solution
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
- B22F3/1025—Removal of binder or filler not by heating only
Abstract
Description
本発明は、結合剤／潤滑剤により結合された粒状物質をプレスすることにより、物品を形成する分野に関し、詳しくは、プレスした後であって焼結する前に、結合剤を除去した高純度焼結物品の部品を製造する方法に関する。
タンタルキャパシタを製造する場合、タンタル粉末と少量の結合剤／潤滑剤とを混合し、その混合物を圧搾成形して必要な形状物を形成し、次に真空中で結合剤が昇華、蒸発、又は分解するように加熱して結合剤を除去することによりアノードを形成するのが典型的である。結合剤を除去した後、アノードを焼結し、粉末を溶融して一体的物品にする。
電気的又は他の高純度用途で、結合剤／潤滑剤材料（以下、結合剤と呼ぶ）の選択は、真空加熱工程後、炭素質残渣が殆ど又は全く残っておらず、除去工程によってアノードに酸素が添加されないようにする必要条件により制約されている。そのような残渣の存在は、焼結タンタル生成物上に付着したアノード酸化物膜を劣化するためキャパシタの電気的性質を変える。現在用いられている結合剤には、樟脳、或るワックス及び或る重合体が含まれる。
これらの結合剤を用いた場合でも、結合剤の不完全な除去又はその分解生成物及び残渣のため、少量の炭素がアノードに付加されることは避けられない。更に、除去のために用いた加熱工程のため、また結合剤自身の中に存在する酸素のため、少量の酸素も存在する。
米国特許第５，４７０，５２５号明細書には、暖かい洗浄剤水溶液中で浸出し、次にきれいな水で洗浄することによりタンタル粉末ペレットから結合剤を除去する方法が記載されている。しかし、上記明細書に開示されている方法では、浸出工程がかなり長い時間、典型的には何時間もかかる。
本発明の目的は、高純度用途のため結合剤を除去する方法で、既知の方法よりも改良された方法を与えることにある。
本発明によれば、プレスした粒状材料から形成した多孔質物品から水不溶性結合剤を除去する方法において、前記結合剤と反応してその水溶性誘導体を生ずる薬品の水溶液と前記物品とを接触させ、それによって前記結合剤誘導体を前記溶液に実質的に溶解することからなる結合剤除去方法が与えられる。
このように、本発明は、化学反応及び高度に溶解性の反応生成物の溶解により結合剤を除去する。この方法で、従来法の複雑な蒸留又は高温加熱処理を用いることなく、既知の加熱浸出法よりもかなり速い速度で結合剤を除去することができる。
接触は、前記薬品を含有又はそれからなる流体中に物品を浸漬することにより行なうことができる。これにより流体が物品の中にそこに存在する気孔を通って入り、結合剤と接触する。
本発明の一つの態様として、物品を薬品の水溶液中に浸漬することにより接触を行なう。
物品からの結合剤の除去を促進するため、水溶液は加熱してもよい。溶液の温度は結合剤の融点よりも高いのが好ましく、それにより溶液中に浸漬した時、結合剤が液化する。
結合剤材料は高級脂肪酸でもよい。この場合変性工程は、その酸をアルカリ性溶液の存在下で加水分解することからなる。これにより脂肪酸の塩が形成され、その塩が、溶液に溶解して結合剤の除去を行う。
好ましい脂肪酸は、ステアリン酸である。脂肪酸は安く、容易に入手でき、非常に効果的な結合剤／潤滑剤である。しかし、今日まで高純度用途のためそれらを使用することは、プレス後、結合剤を完全に除去することは困難であること、及び特にある高純度用途の場合に残渣のため損傷を与えるような炭素含有量が高いことのため、制限されてきた。
本発明の別の態様として、結合剤は水不溶性結合剤材料と水溶性材料との混合物からなる。そのような水溶性材料は、ポリエチレングリコールのような長鎖アルコールである。好ましい組合せはステアリン酸のような脂肪酸とポリエチレングリコールである。ある態様では、脂肪酸５重量％以下を、グリコール５重量％以下に添加する。
ポリエチレングリコールは良好な結合剤であり、脂肪酸は良好な潤滑剤である。一緒にしてそれら２つの成分は、「未焼成（green）」物品の形成に良好な加工性を与える混合物を形成する。
水溶液は、水の中で解離する水酸化物を添加することにより導入された水酸化物イオンを含有する。典型的な例は、水酸化ナトリウム、水酸化カリウム、水酸化アンモニウム等である。
水酸化物は、物品の効果的な浸透を可能にする低い粘度を維持しながら、結合剤との化学量論的反応を確実にする充分な割合で添加すべきである。
流体は、除去工程中撹拌するか、又は別な方法として動かすのがよい。別法として、物品自身を浸漬中動かし、それにより物品中への流体の浸透を促進する。適当な撹拌装置は当業者に知られている。
変性工程が完了したならば、物品中に残留する全ての結合剤誘導体を、奇麗な水で物品を洗うことにより除去する。洗浄工程は変性結合剤の完全な除去が確実に行われるように繰り返す。金属水酸化物溶液を用いた場合、洗浄工程の進行及び効果を、各洗浄溶液の伝導度を測定することにより監視することができる。溶液中に残留する金属イオンは、比較的大きな伝導度の読みを与える。
洗浄後、物品を乾燥し、次に焼結し、固化生成物を形成する。
粒子は金属、例えばニオブ、アルミニウム、タンタル、及びアノード処理可能な他の金属である。一つの態様として、粒子はタンタル粉末からなる。物品をキャパシタのアノードになるように成形する。そのような物品は、大きさが約０．６ｍｍの立方体から直径約６ｍｍ、長さ７ｍｍの円柱までの範囲にある。
本発明は特にタンタルキャパシタの製造に適用され、その場合にタンタル粉末アノードを焼結タンタル粉末から形成し、次にキャパシタに組み込む。そのような製品では、形成されたキャパシタの正確で信頼性のある作動を確実に与えるため、全ての結合剤又は結合剤残渣を、特にアノード表面上に炭素質付着物が形成されるのを抑制することにより除去することが必須である。
次に本発明を実施する方法を単なる例として記述する。
タンタル粉末を少量（５重量％）のステアリン酸［ＣＨ3−（ＣＨ2）16−ＣＯＯＨ］結合剤／潤滑剤と混合する。次に混合物をプレスして成形物品、この例では固体キャパシタのアノード部品を形成する。
次に物品を、約８０℃に加熱した水酸化ナトリウム０．５％水溶液中に約３０分間浸漬し、反応を行わせる。この時間中、物品を撹拌し、溶液が物品の中へ完全に浸透するようにし、更に反応生成物を溶液本体中へ溶解させながら、未反応溶液を物品中へ連続的に導入するようにする。
反応／溶解工程が完了したならば、物品を溶液から取り出し、奇麗な水で洗浄し、物品の気孔中に存在する残留ステアリン酸塩を除去する。洗浄工程は完全に奇麗になるまで繰り返す。各工程後、洗浄溶液の伝導度を慣用的方法により測定し、ナトリウムイオン濃度の指示を与える。ナトリウムイオンが洗浄除去されるに従って、必要な奇麗さが達成されるまで、洗浄溶液の伝導度が低下する。
本発明の別の態様として結合剤はステアリン酸と、平均分子量２０００のポリエチレングリコールからなる。その酸とグリコールは夫々（タンタル重量の％として）４重量％及び０．５重量％で存在する。工程変量の残りは実質的に同じである。
本発明の方法で用いられる処理薬品は比較的危険が少なく、安価であり、環境への影響が少なく、容易に捨てることができる。
本発明による方法で製造されたタンタルアノードは炭素含有量が非常に低い。なぜなら、炭素質物質が実際上完全に除去されているからである。更に、本発明の除去工程で使用される温度が低いため、結合剤除去工程中に付加される酸素の量は無視できる。このため、完成物品の電気的特性は著しく改善されている。特にキャパシタの信頼性は向上し使用中の漏洩電流は減少する。The present invention relates to the field of forming articles by pressing particulate material bound by a binder / lubricant, and in particular, high purity with the binder removed after pressing and before sintering. The present invention relates to a method for manufacturing a component of a sintered article.
When manufacturing tantalum capacitors, tantalum powder and a small amount of binder / lubricant are mixed and the mixture is squeezed to form the required shape, and then the binder is sublimated, evaporated, or The anode is typically formed by heating to decompose to remove the binder. After removal of the binder, the anode is sintered and the powder is melted into an integral article.
For electrical or other high purity applications, the choice of binder / lubricant material (hereinafter referred to as the binder) is such that after the vacuum heating step, little or no carbonaceous residue remains and the removal step results in the anode. Limited by the requirement to prevent oxygen from being added. The presence of such residues changes the electrical properties of the capacitor as it degrades the anodic oxide film deposited on the sintered tantalum product. Currently used binders include camphor, certain waxes and certain polymers.
Even with these binders, it is inevitable that a small amount of carbon is added to the anode due to incomplete removal of the binder or its decomposition products and residues. In addition, small amounts of oxygen are also present due to the heating step used for removal and because of the oxygen present in the binder itself.
U.S. Pat. No. 5,470,525 describes a method for removing binder from tantalum powder pellets by leaching in a warm aqueous detergent solution and then washing with clean water. However, in the method disclosed in the above specification, the leaching process takes a rather long time, typically many hours.
It is an object of the present invention to provide a method that removes the binder for high purity applications and is an improvement over known methods.
According to the present invention, in a method for removing a water-insoluble binder from a porous article formed from a pressed particulate material, the article is contacted with an aqueous solution of a chemical that reacts with the binder to produce a water-soluble derivative thereof. Thereby providing a method of removing the binder comprising substantially dissolving the binder derivative in the solution.
Thus, the present invention removes the binder by chemical reaction and dissolution of the highly soluble reaction product. In this way, the binder can be removed at a much faster rate than the known heat leaching method without using the complex distillation or high temperature heat treatment of conventional methods.
Contact can be effected by immersing the article in a fluid containing or consisting of the drug. This allows fluid to enter the article through the pores present therein and contact the binder.
In one embodiment of the invention, the contact is made by immersing the article in an aqueous solution of the chemical.
The aqueous solution may be heated to facilitate the removal of the binder from the article. The temperature of the solution is preferably higher than the melting point of the binder, so that the binder liquefies when immersed in the solution.
The binder material may be a higher fatty acid. In this case, the modification step consists of hydrolyzing the acid in the presence of an alkaline solution. This forms a fatty acid salt which dissolves in the solution and removes the binder.
A preferred fatty acid is stearic acid. Fatty acids are cheap, readily available and a very effective binder / lubricant. However, using them for high-purity applications to date makes it difficult to completely remove the binder after pressing, and may cause damage due to residue, especially in certain high-purity applications Limited due to the high carbon content.
In another embodiment of the invention, the binder comprises a mixture of a water insoluble binder material and a water soluble material. Such water soluble materials are long chain alcohols such as polyethylene glycol. A preferred combination is a fatty acid such as stearic acid and polyethylene glycol. In some embodiments, 5 wt% or less of the fatty acid is added to 5 wt% or less of the glycol.
Polyethylene glycol is a good binder and fatty acids are good lubricants. Together, the two components form a mixture that gives good processability to the formation of “green” articles.
The aqueous solution contains hydroxide ions introduced by adding a hydroxide that dissociates in water. Typical examples are sodium hydroxide, potassium hydroxide, ammonium hydroxide and the like.
The hydroxide should be added in a sufficient proportion to ensure a stoichiometric reaction with the binder while maintaining a low viscosity that allows effective penetration of the article.
The fluid may be stirred during the removal process or otherwise moved. Alternatively, the article itself is moved during immersion, thereby facilitating fluid penetration into the article. Suitable agitation devices are known to those skilled in the art.
Once the denaturation step is complete, any binder derivative remaining in the article is removed by washing the article with clean water. The washing process is repeated to ensure complete removal of the modified binder. When a metal hydroxide solution is used, the progress and effect of the cleaning process can be monitored by measuring the conductivity of each cleaning solution. Metal ions remaining in solution give a relatively large conductivity reading.
After washing, the article is dried and then sintered to form a solidified product.
The particles are metals such as niobium, aluminum, tantalum, and other metals that can be anodized. In one embodiment, the particles consist of tantalum powder. The article is shaped to be the capacitor anode. Such articles range from a cube with a size of about 0.6 mm to a cylinder with a diameter of about 6 mm and a length of 7 mm.
The invention is particularly applicable to the manufacture of tantalum capacitors, where the tantalum powder anode is formed from sintered tantalum powder and then incorporated into the capacitor. In such a product, all binders or binder residues are suppressed, especially the formation of carbonaceous deposits on the anode surface, to ensure accurate and reliable operation of the formed capacitor. It is essential to remove it.
The method of practicing the present invention will now be described by way of example only.
Tantalum powder is mixed with a small amount (5% by weight) of stearic acid [CH 3 — (CH 2 ) 16 —COOH] binder / lubricant. The mixture is then pressed to form a molded article, in this example a solid capacitor anode part.
The article is then immersed in a 0.5% aqueous sodium hydroxide solution heated to about 80 ° C. for about 30 minutes to allow the reaction to occur. During this time, the article is agitated so that the solution completely penetrates into the article and the unreacted solution is continuously introduced into the article while dissolving the reaction product into the solution body. .
When the reaction / dissolution process is complete, the article is removed from the solution and washed with clean water to remove residual stearate present in the pores of the article. The washing process is repeated until it is completely clean. After each step, the conductivity of the cleaning solution is measured by conventional methods and an indication of sodium ion concentration is given. As the sodium ions are washed away, the conductivity of the washing solution decreases until the required cleanliness is achieved.
In another embodiment of the present invention, the binder comprises stearic acid and polyethylene glycol having an average molecular weight of 2000. The acid and glycol are present in 4 wt% and 0.5 wt% (as% of tantalum weight), respectively. The rest of the process variables are substantially the same.
The treatment chemicals used in the method of the present invention are relatively less dangerous, inexpensive, have little environmental impact, and can be easily discarded.
The tantalum anode produced by the method according to the invention has a very low carbon content. This is because the carbonaceous material is practically completely removed. Furthermore, since the temperature used in the removal process of the present invention is low, the amount of oxygen added during the binder removal process is negligible. For this reason, the electrical properties of the finished article are significantly improved. In particular, the reliability of the capacitor is improved and the leakage current during use is reduced.
Claims (6)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB9700566.4 | 1997-01-13 | ||
| GBGB9700566.4A GB9700566D0 (en) | 1997-01-13 | 1997-01-13 | Binder removal |
| PCT/GB1998/000023 WO1998030348A1 (en) | 1997-01-13 | 1998-01-06 | Binder removal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001508128A JP2001508128A (en) | 2001-06-19 |
| JP4230541B2 true JP4230541B2 (en) | 2009-02-25 |
Family
ID=10805885
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP53062998A Expired - Fee Related JP4230541B2 (en) | 1997-01-13 | 1998-01-06 | Binder removal method |
Country Status (12)
| Country | Link |
|---|---|
| US (1) | US6197252B1 (en) |
| EP (1) | EP0951374B1 (en) |
| JP (1) | JP4230541B2 (en) |
| KR (1) | KR100494140B1 (en) |
| CN (1) | CN1106898C (en) |
| AT (1) | ATE223274T1 (en) |
| AU (1) | AU5490498A (en) |
| DE (1) | DE69807650T2 (en) |
| GB (1) | GB9700566D0 (en) |
| IL (1) | IL130892A (en) |
| PT (1) | PT951374E (en) |
| WO (1) | WO1998030348A1 (en) |
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1998
- 1998-01-06 DE DE69807650T patent/DE69807650T2/en not_active Expired - Lifetime
- 1998-01-06 CN CN98801795A patent/CN1106898C/en not_active Expired - Fee Related
- 1998-01-06 PT PT98900293T patent/PT951374E/en unknown
- 1998-01-06 EP EP98900293A patent/EP0951374B1/en not_active Expired - Lifetime
- 1998-01-06 WO PCT/GB1998/000023 patent/WO1998030348A1/en active IP Right Grant
- 1998-01-06 AT AT98900293T patent/ATE223274T1/en not_active IP Right Cessation
- 1998-01-06 JP JP53062998A patent/JP4230541B2/en not_active Expired - Fee Related
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- 1998-01-06 IL IL13089298A patent/IL130892A/en not_active IP Right Cessation
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1999
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| KR20000070086A (en) | 2000-11-25 |
| DE69807650T2 (en) | 2003-04-24 |
| IL130892A0 (en) | 2001-01-28 |
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| PT951374E (en) | 2003-01-31 |
| ATE223274T1 (en) | 2002-09-15 |
| EP0951374A1 (en) | 1999-10-27 |
| DE69807650D1 (en) | 2002-10-10 |
| KR100494140B1 (en) | 2005-06-10 |
| EP0951374B1 (en) | 2002-09-04 |
| WO1998030348A1 (en) | 1998-07-16 |
| GB9700566D0 (en) | 1997-03-05 |
| US6197252B1 (en) | 2001-03-06 |
| JP2001508128A (en) | 2001-06-19 |
| CN1243464A (en) | 2000-02-02 |
| CN1106898C (en) | 2003-04-30 |
| IL130892A (en) | 2002-12-01 |
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